EP0321925A2 - Apparatus for analysis employing electron - Google Patents
Apparatus for analysis employing electron Download PDFInfo
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- EP0321925A2 EP0321925A2 EP88121303A EP88121303A EP0321925A2 EP 0321925 A2 EP0321925 A2 EP 0321925A2 EP 88121303 A EP88121303 A EP 88121303A EP 88121303 A EP88121303 A EP 88121303A EP 0321925 A2 EP0321925 A2 EP 0321925A2
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- specimen
- oil
- purge gas
- vacuum pump
- sealed rotary
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
Definitions
- the present invention relates to an apparatus for analysis which employs electron and in which rotary vacuum pump evacuates gas or air from a specimen exchange chamber, and, more particularly, to an apparatus for analysis which employs electron and in which the evacuated side of the apparatus is prevented from being contaminated by a vacuum pump oil.
- an object of the present invention is to provide an analysis apparatus in which high degrees of the cleanliness and vacuum of a specimen chamber are maintained.
- Another object of the present invention is to provide an analysis apparatus with which analysis or observation can be continued for long period.
- Another object of the present invention is to provide an analysis apparatus which makes a high degree of resolution in analysis possible.
- Another object of the present invention is to provide an analysis apparatus in which the interior of the specimen chamber is made clean by a simple additional equipment.
- the above-described object of the present invention regarding the apparatus for analysis employing electron and having the specimen chamber from which air is evacuated by an oil-sealed rotary vacuum pump can be attained by that on the upstream side of the oil-sealed rotary vacuum pump, a purge gas supplying means is arranged, the purge gas supplying means supplying a small quantity of purge gas while the air is evacuated from the specimen exchange chamber by the ultimate pressure of the pump.
- the purge gas is supplied by the purge gas supplying means arranged on the upstream side of the oil-sealed rotary vacuum pump when air in the specimen exchange chamber in the analysis apparatus employing electron is evacuated to the ultimate pressure of the vacuum pump, the quantity of supplied purge gas being regulated at the minimum degree needed to prevent the oil used in the oil-sealed rotary vacuum pump from flowing backward to the inlet side thereof. In consequence, the backstreaming of the oil of the vacuum pump toward the specimen exchange chamber can be suppressed by this purge gas.
- the supplied quantity of purge gas is about one tenth in comparison with the purge gas supplied in the conventional purging method, so that a clean vacuum state can be provided without an increase in the ultimate pressure of the vacuum evacuation system, thereby an apparatus for analysis employing electron in which the oil contamination of the evacuation system is suppressed, is provided.
- a scanning electron microscope 1 includes a microscope column 2 and a specimen chamber 3 formed below the microscope column 2.
- the microscope column 2 incorporates an electron gun 4 and an electron lens system which consists of a first condenser lens 5, a second condenser lens 6, an objective lens 7, and a deflection system of electron beam 8 for deflecting a focussed electron beam on a specimen during scanning operation.
- the specimen chamber 3 is provided with a specimen exchange chamber 10 from which a specimen 9 is delivered into the specimen chamber 3, the specimen exchange chamber 10 being connected to the specimen chamber 3 through a gate valve 11.
- the microscope column 2 is equipped with a main pumping system constituted by three ultra-high vacuum pumps 12A to 12C, and three roughing pipes 13A to 13C for roughing the interior of the microscope column 2 are coupled to the microscope column 2.
- the three roughing pipes 13A to 13C are respectively provided with a first roughing valve 14A, a second roughing valve 14B and a third roughing valve 14C.
- the roughing pipes 13A to 13C are connected to a roughing pipe 15 which is connected to one end of a manifold 17 through a manifold valve 16.
- the manifold 17 communicates with the specimen chamber 3 through specimen chamber exhausting pipes 18A to 18C.
- the manifold 17 is provided with a Pirani gauge 19 for measuring a roughing pressure, a Penning gauge 20 for measuring a main vacuum pumping pressure, and a leak valve 21 through which gas is inserted into the microscope column 2.
- Another end of the manifold 17 is connected through a manifold gate valve 22 and a cold trap 23 to a turbo molecular pump 24 which acts as a roughing vacuum pumping pump.
- the outlet of the turbo molecular pump 24 is connected through a suction pipe 25 to a first oil-sealed rotary vacuum pump 26.
- a valve 27 for the first oil-sealed rotary vacuum pump 26 is arranged between the suction pipe 25 and the first oil-sealed rotary vacuum pump 26, and a leak valve 28 through which gas is inserted into the suction pipe 25 is arranged on the suction pipe 25.
- a outlet pipe 29 for the first oil-sealed rotary vacuum pump 26 and a outlet pipe 31 for a second oil-sealed rotary vacuum pipe 30 join into one pipe.
- the second oil-sealed rotary vacuum pump 30 evacuates air principally from the specimen exchange chamber 10.
- the second oil-sealed rotary vacuum pump 30 has a suction pipe 32, which is coupled to the specimen exchange chamber 10 through a stop valve 33.
- a pirani gauge 34 for measuring the pressure and a leak valve 35 through which gas is inserted into the suction pipe 32 are arranged between the stop valve 33 and the specimen exchange chamber on the suction pipe 32.
- the portion of the suction pipe 32 between the stop valve 33 and the second oil-sealed rotary vacuum pump 30 communicated with the another end of the manifold 17 through a bypass pipe 36 which is provided with a bypass valve 37.
- the portion of the suction pipe 32 between the stop valve 33 and the second oil-sealed rotary vacuum pump 30 is provided with a leak valve 38.
- the portion of the suction pipe 32 between the inlet of the second oil-sealed rotary vacuum pump 30 and the leak valve 38 is provided with a purge gas supply means 40 for supplying a small quantity of purge gas.
- the purge gas supply means 40 includes a purge gas pipe 41 one end of which is open to the atmosphere and another end of which is connected to the suction pipe 32 for the second oil-sealed rotary vacuum pump 30, a microflow rate adjusting orifice 42 which is arranged on the purge as pipe 41 and which limits a quantity of gas flowing through the purge gas pipe 41, and a filter 43 arranged on the purge gas pipe 41 between the orifice 42 and the atomosphere.
- the first roughing valve 14A, the second roughing valve 14B, the third roughing valve 14C, the manifold valve 16, the manifold gate valve 22, and the valve 27 for the first oil-sealed rotary vacuum pump 26 are opened, the leak valve 21, the leak valve 28, the leak valve 38, the bypass valve 37, the gate valve 11, and the stop valve 33 are closed, and the first and second oil-sealed rotary vacuum pumps 26 and 30 are operated to evacuate air from the microscope column 2 and from a part of the suction pipe 32 between the stop valve 33 and the second oil-sealed rotary vacuum pump 30.
- the pressure in the manifold 17 is measured with the Pirani gauge 19 arranged in the manifold 17.
- the turbo molecular pump 24 is operated to evacuate air in cooperation with the first oil-sealed rotary vacuum pump 26.
- the pressure in the manifold 17 is measured with the Penning gauge 20 arranged in the manifold 17.
- the ion pumps 12A to 12C are operated for main pumping. After the main pumping has been finished, the specimen 9 in the specimen chamber 3 is scanned. After the scanning of the specimen 9 is performed, a new specimen is set into the specimen exchange chamber to replace the specimen 9 which has been scanned.
- the stop valve 33 is opened, and the air in the specimen exchange chamber 10 is evacuated.
- the stop valve 33 is closed.
- the gate valve 11 is opened, the specimen 9 is replaced, and the gate valve 11 is closed.
- the air in the microscope column 2 is again evacuated to a predetermined pressure, and scanning is then performed.
- gas is inserted into the specimen exchange chamber 10 through the leak valve 35 so as to make the pressure in the specimen exchange chamber 10 equal to the atmospheric pressure, and a subsequent specimen 9 is then set, thereby one cycle of analysis by the scanning electron microscope is performed.
- the purge gas supply means 40 supplies a small quantity of purge gas to the inlet side of the second oil-sealed rotary vacuum pump 30 while the air in the specimen exchange chamber 10 is evacuated by the second oil-sealed rotary vacuum pump 30.
- the present embodiment employs clean air which has been passed through the filter 43.
- the air passes through the filter 43, the orifice 42, and the purge gas pipe 41, and is supplied to the inlet side of the second oil-sealed rotary vacuum pump 30.
- a chemically stable inert gas is preferable as a purge gas.
- nitrogen gas or clean air which contains no oil may be also effective.
- Table 1 shows the results of the experiments.
- Table 1 Type of gas Quantity of gas for effective purging * (SCCM) Nitrogen gas (N2) 0.6 Helium gas (He) 12.7 Argon gas (Ar) 0.4 *) The quantity of gas for effective purging as shown in Table 1 was measured, when the oil contained in the gas evacuated with purging became about one hundredth in comparison with the oil in the gas evacuated without purging.
- Fig. 2 is a mass spectrum of the residual gas collected at the inlet side of the second oil-sealed rotary vacuum pump 30 when the second oil-sealed rotary vacuum pump 30 was operated at the almost ultimate pressure of the pump and the purging gas was inserted in the inlet side of the pump.
- the residual gas was analyzed by a quadpole mass spectrometer.
- the ordinate represents degree of the ion current, and the abscissa represents degree of the mass number.
- Fig. 2 shows that a very clean state was provided.
- Fig. 3 is a mass spectrum of the residual gas collected at the inlet side of the second oil-sealed rotary vacuum pump 30 when no purging gas was inserted.
- a large number of peaks corresponding to the (hydrocarbon) components of the oil used in the second oil-sealed rotary vacuum pump 30 are shown in a range of mass number larger than 39. From the above fact, it can be understood that oil backstreaming increased at a high degree in that range.
- Fig. 4 shows the result of the experiment for making clear the relation among the purged quantity of nitrogen gas, the quantities of components of the residual gas and the pressure at the inlet of the second vacuum pump 39 (hereinafter referred to simply as the inlet pressure).
- the ordinate on the left side represents degree of the ion current for the detected peaks of the residual gas components
- the ordinate on the right side represents degree of the inlet pressure
- the abscissa represents degree of the purged gas.
- the quantity of purge gas is about 0.6 SCCM the peak values of the hydrocarbon components of the oil used in the oil-sealed rotary vacuum pump decrease by ninety-nine percent in comparison with the case of no-purging.
- the peaks of the hydrocarbon components decrease in proportion to the increase of purge gas.
- the amount of purge gas exceeds more than about 4 SCCM, there is substantially no change in the peak values of the hydrocarbon components and in the decrease of the backstreaming of the oil, and the vacuum pressure by the pump increases.
- the quantity of the purge gas is suitable for the quantity of the purge gas to be within a range from about 0.3 SCCM to about 4 SCCM, because at about 0.3 SCCM, the peak values of the hydrocarbon components reduce to about one tenth in comparison with the case of no purging and because at more than about 4 SCCM, the values of in the peaks of the hydrocarbon components are substantially constant. Under such a purging condition, it is possible for the suction pressure of the pump to be about 7.5 x 10 ⁇ 3 Torr to 2.5 x 10 ⁇ 2 Torr.
- Fig. 4 shows, when a small quantity of purge gas is supplied each peak value of component of the oil contained in the evacuated air is about one hundredth in comparison with the case of no purging, so that a clean vacuum state is provided.
- the quantity of purge gas according to the present invention is very small in comparison with the conventional purging method.
- the quantity of purge gas according to the present invention will be compared with the quantity of purge gas according to the conventional purging method under the condition that the oil-sealed rotary vacuum pump evacuates by 240 l/min.
- the ultimate pressure of the vacuum pumping system according to the present invention can be lower than the pressure of 13 Pa (0.1 Torr) provided by the conventional purging method, and the vacuum state can be clean.
- the interior of the specimen chamber 3 can be made clean by the supply of a very small quantity of purge gas will be explained below. That is, according to the analysis: although the change in the pressure caused by the supply of a small quantity of purge gas is small, by the supply of the purge gas the Knudsen number increases, and the state of the evacuated flow changes from a molecular flow to an intermediate flow. As the result, the frequency in collision between the oil particles and the purge gas particles increases substantially, so that the backstreaming of the oil is impeded remarkably.
- the supply of purging gas generates a flow toward the vacuum pump, and the oil particles are carried thereto.
- a vacuum state in which the oil contamination is decreased is provided by slight reconstructions of equipments used in the vacuum system.
- Fig. 5 shows a second embodiment of the present invention in which the present invention is applied to a scanning electron microscope.
- the purge gas supply means 40 includes a mass flow controller 44 for controlling a flow rate of purge gas, instead of the orifice 42 included in the means 40 in the first embodiment.
- the amount of purge gas does not change if the pressure at the inlet of the mass flow controller changes, so that the variation of pressure in vacuum system is very small.
- Fig. 6 shows a third embodiment of the present invention in which the present invention is applied to a scanning electron microscope.
- the purge gas supply means 40 includes a microflow supply valve 45, a microflow meter 46, a purge gas source 47 and a purge gas pipe 41, and the purge gas is supplied not from the atmosphere but from the purge gas source 47.
- the main components of residual gas are supplied from the purge gas source 47, so that the specimen can be surrounded by a desired gas as shown in Fig. 4.
- Fig. 7 shows a fourth embodiment of the present invention in which the present invention is applied to a scanning electron microscope.
- the purge gas supply means 40 includes a microflow meter 46 which operates as a purging checker for checking whether or not a purge gas is flowing.
- the microflow meter 46 generates a signal for closing the manifold gate valve 22, the bypass valve 37 and the stop valve 33 when the quantity of purge gas is less than a predetermined level so that the oil contamination is prevented.
- the generated signal is transmitted through a valve control signal line 48. This system improves the reliability of the system.
- Fig. 8 shows a fifth embodiment of the present invention in which the present invention is applied to a scanning electron microscope.
- This embodiment employs a Pirani gauge 34 as the purging checker.
- the vacuum pressure which is the predetermined value or below is detected by the Pirani gauge 34 arranged in the suction pipe 32 between the specimen exchange chamber and the second vacuum pump 30, and the Pirani gauge 34 generates a signal to close the manifold gate valve 22, the bypass valve 37, and the stop valve 33.
- the state in the inlet side of the second vacuum pump 30 is checked, so the reliability of the system is improved.
- Fig. 9 shows a sixth embodiment of the present invention in which the present invention is applied to a scanning electron microscope.
- This embodiment includes, as a purging checker, optical fiber cables 49 for detecting the clogging of the microflow orifice 42, and a detector 50 for judging whether the orifice clogs up or not and for generating a signal to open or close the valves.
- the optical fibers 49 face each other at an end of the microflow orifice 42. A ray of light inserted into an end of the optical fiber 49 is detected by the detector 50 when the purge gas flows through the orifice 42. However, if the microflow orifice 42 is clogged by a foreign substance, the ray of light is interrupted, and no light is detected by the detector 50.
- the detector 50 judges whether the orifice clogs up or not and generates the signal for closing the manifold gate valve 22, the bypass valve 37 and the stop valve 33. In this embodiment, the clogging of the microflow orifice 42 is always monitored, so that the reliability of the system is improved.
- Fig. 10 shows a seventh embodiment of the present invention in which the present invention is applied to a scanning electron microscope.
- This embodiment includes a purge gas supply means 40 for supplying a controlled quantity of purge gas to the inlet side of the second oil-sealed rotary vacuum pump 30 according to the pressure of the inlet side of the second oil-sealed rotary vacuum pump 30.
- the purge gas supply means 40 in this embodiment includes a microflow supply valve 45, a microflow meter 46, a purge gas source 47, a pressure signal line 52, a microflow valve control signal line 53 and a microflow valve controller 51.
- the Pirani gauge 34 measures the pressure of the inlet side of the second oil-sealed rotary vacuum pump 30, generates a signal in accordance with the measured pressure and transmits the signal through the pressure signal line 52 to the microflow valve controller 51.
- the microflow valve controller 51 According to the transmitted signal, the microflow valve controller 51 generates and transmits a signal for controlling the opening degree of the microflow supply valve 45 through the microflow valve control signal line 53 to the microflow supply valve 45 so that the opening degree of the microflow supply valve 45 increases or decreases in accordance with a difference between the measured pressure and the predetermined pressure.
- the microflow valve controller 51 When the measured pressure is larger than the predetermined pressure, the microflow valve controller 51 generates the signal for decreasing the opening degree of the microflow supply valve 45.
- the microflow valve controller 51 When the measured pressure is smaller than the predetermined pressure, the microflow valve controller 51 generates the signal for increasing the opening degree of the microflow supply valve 45. When the measured pressure is equal to the predetermined pressure, the microflow valve controller 51 generates the signal for maintaining the opening degree of the microflow supply valve 45 as it is. As described above, the pressure of the inlet side of the second oil-sealed rotary vacuum pump 30 is maintained within a suitable range. As in this embodiment the quantity of the supplied purge gas is automatically controlled, the reriability and economical efficiency of the system are improved.
- the present invention is applied to a scanning electron microscope.
- the present invention can also be applied to a transmission type electron microscope, a mass spectrometer or an ion microanalyzer.
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Abstract
Description
- The present invention relates to an apparatus for analysis which employs electron and in which rotary vacuum pump evacuates gas or air from a specimen exchange chamber, and, more particularly, to an apparatus for analysis which employs electron and in which the evacuated side of the apparatus is prevented from being contaminated by a vacuum pump oil.
- Means for preventing the interior of a vacuum chamber in a vacuum system from being contaminated by an oil backstreaming from a vacuum pump employing oil is described on pages 299 to 307 of THE JOURNAL OF VACUUM SCIENCE AND TECHNOLOGY, VOL. 8, No. 1 (issued in 1971). In a method described in this publication, on the basis of the fact that oil contamination increases rapidly when the pressure at the inlet of the oil-sealed rotary vacuum pump decreases below 13 Pa (0.1 Torr), a dried nitrogen purging portion is arranged at the inlet of the oil-sealed rotary vacuum pump and prevents the pressure of the inlet from decreasing below a level from 13 to 40 Pa (0.1 to 0.3 Torr)
- The increase in magnification of analysis systems which employ electron such as electron microscopes has been advanced in recent years, but the further increase has been arrested by the contamination of microscope columns by an oil backstreaming from the oil-sealed rotary vacuum pumps used to evacuate air from specimen exchange chambers. Particularly, when an oil-sealed rotary vacuum pump operates at the almost ultimate pressure of the pump, this backstreaming of oil becomes a high degree. However, the above-described conventional purging method maintains the pressure of the inlet of the vacuum pump above 13 Pa (0.1 Torr) by purging in order to prevent the interior of the vacuum chamber from being contaminated by the oil backstreaming to the vacuum chamber from the oil-sealed rotary vacuum pump. So, when this conventional purging method is applied to the electron microscope, the pressure in the specimen chamber from which unnecessary gas has been evacuated is a high degree, so that the pressure in the specimen chamber is not be decreased below 13 Pa (0.1 Torr) in order to maintain the clean environment of the specimen chamber.
- Accordingly, an object of the present invention is to provide an analysis apparatus in which high degrees of the cleanliness and vacuum of a specimen chamber are maintained.
- Another object of the present invention is to provide an analysis apparatus with which analysis or observation can be continued for long period.
- Another object of the present invention is to provide an analysis apparatus which makes a high degree of resolution in analysis possible.
- Another object of the present invention is to provide an analysis apparatus in which the interior of the specimen chamber is made clean by a simple additional equipment.
- The above-described object of the present invention regarding the apparatus for analysis employing electron and having the specimen chamber from which air is evacuated by an oil-sealed rotary vacuum pump, can be attained by that on the upstream side of the oil-sealed rotary vacuum pump, a purge gas supplying means is arranged, the purge gas supplying means supplying a small quantity of purge gas while the air is evacuated from the specimen exchange chamber by the ultimate pressure of the pump.
- In the present invention, the purge gas is supplied by the purge gas supplying means arranged on the upstream side of the oil-sealed rotary vacuum pump when air in the specimen exchange chamber in the analysis apparatus employing electron is evacuated to the ultimate pressure of the vacuum pump, the quantity of supplied purge gas being regulated at the minimum degree needed to prevent the oil used in the oil-sealed rotary vacuum pump from flowing backward to the inlet side thereof. In consequence, the backstreaming of the oil of the vacuum pump toward the specimen exchange chamber can be suppressed by this purge gas. At this time, the supplied quantity of purge gas is about one tenth in comparison with the purge gas supplied in the conventional purging method, so that a clean vacuum state can be provided without an increase in the ultimate pressure of the vacuum evacuation system, thereby an apparatus for analysis employing electron in which the oil contamination of the evacuation system is suppressed, is provided.
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- Fig. 1 is a schematic view of a scanning electron microscope, showing a first embodiment of the present invention;
- Fig. 2 is a mass spectrum of residual gas collected at the upstream side of the oil-sealed rotary vacuum pump of the apparatus for analysis when the purge gas is supplied;
- Fig. 3 shows a mass spectrum of residual gas collected at the upstream side of the oil-sealed rotary vacuum pump of the apparatus for analysis when the purge gas is not supplied;
- Fig. 4 shows the relationship among the amount of the purge gas, the spectral peaks of the residual gas components and the pressure at the inlet of the pump;
- Figs. 5 to 10 respectively show second, third, fourth, fifth, sixth and seventh embodiments of the present invention which is applied to electron microscopes.
- The embodiments according to the present invention will be described below with the accompanying drawings thereof in which a scanning electron microscope is shown as an apparatus for analysis employing electron.
- In Fig. 1 which shows a first embodiment of the scanning electron microscope to which the present invention is applied, a scanning electron microscope 1 includes a
microscope column 2 and aspecimen chamber 3 formed below themicroscope column 2. Themicroscope column 2 incorporates anelectron gun 4 and an electron lens system which consists of afirst condenser lens 5, asecond condenser lens 6, anobjective lens 7, and a deflection system ofelectron beam 8 for deflecting a focussed electron beam on a specimen during scanning operation. Thespecimen chamber 3 is provided with aspecimen exchange chamber 10 from which a specimen 9 is delivered into thespecimen chamber 3, thespecimen exchange chamber 10 being connected to thespecimen chamber 3 through a gate valve 11. - Next, a vacuum pumping system for evacuating air from the interiors of the
microscope column 2, thespecimen chamber 3 and thespecimen exchange chamber 10 will be described below. Themicroscope column 2 is equipped with a main pumping system constituted by threeultra-high vacuum pumps 12A to 12C, and three roughingpipes 13A to 13C for roughing the interior of themicroscope column 2 are coupled to themicroscope column 2. The three roughingpipes 13A to 13C are respectively provided with a first roughingvalve 14A, a second roughingvalve 14B and a third roughingvalve 14C. The roughingpipes 13A to 13C are connected to a roughingpipe 15 which is connected to one end of amanifold 17 through amanifold valve 16. Themanifold 17 communicates with thespecimen chamber 3 through specimen chamberexhausting pipes 18A to 18C. Themanifold 17 is provided with a Piranigauge 19 for measuring a roughing pressure, aPenning gauge 20 for measuring a main vacuum pumping pressure, and aleak valve 21 through which gas is inserted into themicroscope column 2. Another end of themanifold 17 is connected through amanifold gate valve 22 and acold trap 23 to a turbomolecular pump 24 which acts as a roughing vacuum pumping pump. The outlet of the turbomolecular pump 24 is connected through asuction pipe 25 to a first oil-sealedrotary vacuum pump 26. Avalve 27 for the first oil-sealedrotary vacuum pump 26 is arranged between thesuction pipe 25 and the first oil-sealedrotary vacuum pump 26, and aleak valve 28 through which gas is inserted into thesuction pipe 25 is arranged on thesuction pipe 25. Aoutlet pipe 29 for the first oil-sealedrotary vacuum pump 26 and aoutlet pipe 31 for a second oil-sealedrotary vacuum pipe 30 join into one pipe. The second oil-sealedrotary vacuum pump 30 evacuates air principally from thespecimen exchange chamber 10. The second oil-sealedrotary vacuum pump 30 has asuction pipe 32, which is coupled to thespecimen exchange chamber 10 through astop valve 33. Apirani gauge 34 for measuring the pressure and aleak valve 35 through which gas is inserted into thesuction pipe 32 are arranged between thestop valve 33 and the specimen exchange chamber on thesuction pipe 32. The portion of thesuction pipe 32 between thestop valve 33 and the second oil-sealedrotary vacuum pump 30 communicated with the another end of themanifold 17 through abypass pipe 36 which is provided with abypass valve 37. The portion of thesuction pipe 32 between thestop valve 33 and the second oil-sealedrotary vacuum pump 30 is provided with aleak valve 38. The portion of thesuction pipe 32 between the inlet of the second oil-sealedrotary vacuum pump 30 and theleak valve 38 is provided with a purge gas supply means 40 for supplying a small quantity of purge gas. The purge gas supply means 40 includes apurge gas pipe 41 one end of which is open to the atmosphere and another end of which is connected to thesuction pipe 32 for the second oil-sealedrotary vacuum pump 30, a microflowrate adjusting orifice 42 which is arranged on the purge aspipe 41 and which limits a quantity of gas flowing through thepurge gas pipe 41, and afilter 43 arranged on thepurge gas pipe 41 between theorifice 42 and the atomosphere. - The operation of the first embodiment will be described below. After the specimen 9 has been set in the
specimen chamber 3, thefirst roughing valve 14A, thesecond roughing valve 14B, thethird roughing valve 14C, themanifold valve 16, themanifold gate valve 22, and thevalve 27 for the first oil-sealedrotary vacuum pump 26 are opened, theleak valve 21, theleak valve 28, theleak valve 38, thebypass valve 37, the gate valve 11, and thestop valve 33 are closed, and the first and second oil-sealedrotary vacuum pumps microscope column 2 and from a part of thesuction pipe 32 between thestop valve 33 and the second oil-sealedrotary vacuum pump 30. The pressure in themanifold 17 is measured with the Piranigauge 19 arranged in themanifold 17. When the pressure in themanifold 17 has reached a predetermined pressure, the turbomolecular pump 24 is operated to evacuate air in cooperation with the first oil-sealedrotary vacuum pump 26. The pressure in themanifold 17 is measured with thePenning gauge 20 arranged in themanifold 17. When it has reached a predetermined pressure, theion pumps 12A to 12C are operated for main pumping. After the main pumping has been finished, the specimen 9 in thespecimen chamber 3 is scanned. After the scanning of the specimen 9 is performed, a new specimen is set into the specimen exchange chamber to replace the specimen 9 which has been scanned. Subsequently, thestop valve 33 is opened, and the air in thespecimen exchange chamber 10 is evacuated. After theleak valve 35 has been closed and the air in thespecimen exchange chamber 10 has been evacuated to a predetermined pressure, thestop valve 33 is closed. Subsequently, the gate valve 11 is opened, the specimen 9 is replaced, and the gate valve 11 is closed. The air in themicroscope column 2 is again evacuated to a predetermined pressure, and scanning is then performed. During this time, gas is inserted into thespecimen exchange chamber 10 through theleak valve 35 so as to make the pressure in thespecimen exchange chamber 10 equal to the atmospheric pressure, and a subsequent specimen 9 is then set, thereby one cycle of analysis by the scanning electron microscope is performed. - When the air in the
specimen exchange chamber 10 is evacuated by the second oil-sealedrotary vacuum pump 30 at the substantially ultimate pressure of the vacuum pump, the backstreaming of oil rapidly increases, contaminating thespecimen exchange chamber 10 and the specimen 9. Further, when the gate valve 11 is opened, a stream flows from thespecimen exchange chamber 10 to thespecimen chamber 3 due to the difference in pressure between thespecimen chamber 3 and thespecimen exchange chamber 10, so that the oil contamination of thespecimen exchange chamber 10 spreads into thespecimen chamber 3. In order to suppress this oil contamination, the purge gas supply means 40 supplies a small quantity of purge gas to the inlet side of the second oil-sealedrotary vacuum pump 30 while the air in thespecimen exchange chamber 10 is evacuated by the second oil-sealedrotary vacuum pump 30. The present embodiment employs clean air which has been passed through thefilter 43. The air passes through thefilter 43, theorifice 42, and thepurge gas pipe 41, and is supplied to the inlet side of the second oil-sealedrotary vacuum pump 30. A chemically stable inert gas is preferable as a purge gas. However, nitrogen gas or clean air which contains no oil may be also effective. In the experiments, it was found that the larger the molecular weight of the gas to be supplied is the more the amount of the gas can be reduced. Table 1 shows the results of the experiments.Table 1 Type of gas Quantity of gas for effective purging *) (SCCM) Nitrogen gas (N₂) 0.6 Helium gas (He) 12.7 Argon gas (Ar) 0.4 *) The quantity of gas for effective purging as shown in Table 1 was measured, when the oil contained in the gas evacuated with purging became about one hundredth in comparison with the oil in the gas evacuated without purging. - Fig. 2 is a mass spectrum of the residual gas collected at the inlet side of the second oil-sealed
rotary vacuum pump 30 when the second oil-sealedrotary vacuum pump 30 was operated at the almost ultimate pressure of the pump and the purging gas was inserted in the inlet side of the pump. The residual gas was analyzed by a quadpole mass spectrometer. The ordinate represents degree of the ion current, and the abscissa represents degree of the mass number. Fig. 2 shows that a very clean state was provided. - Fig. 3 is a mass spectrum of the residual gas collected at the inlet side of the second oil-sealed
rotary vacuum pump 30 when no purging gas was inserted. In Fig. 3, a large number of peaks corresponding to the (hydrocarbon) components of the oil used in the second oil-sealedrotary vacuum pump 30 are shown in a range of mass number larger than 39. From the above fact, it can be understood that oil backstreaming increased at a high degree in that range. - Fig. 4 shows the result of the experiment for making clear the relation among the purged quantity of nitrogen gas, the quantities of components of the residual gas and the pressure at the inlet of the second vacuum pump 39 (hereinafter referred to simply as the inlet pressure). The ordinate on the left side represents degree of the ion current for the detected peaks of the residual gas components, the ordinate on the right side represents degree of the inlet pressure, and the abscissa represents degree of the purged gas. In Fig. 4, when the quantity of purge gas is about 0.6 SCCM the peak values of the hydrocarbon components of the oil used in the oil-sealed rotary vacuum pump decrease by ninety-nine percent in comparison with the case of no-purging. As the quantity of purge gas increases further, the peaks of the hydrocarbon components decrease in proportion to the increase of purge gas. When the amount of purge gas exceeds more than about 4 SCCM, there is substantially no change in the peak values of the hydrocarbon components and in the decrease of the backstreaming of the oil, and the vacuum pressure by the pump increases. Practically it is suitable for the quantity of the purge gas to be within a range from about 0.3 SCCM to about 4 SCCM, because at about 0.3 SCCM, the peak values of the hydrocarbon components reduce to about one tenth in comparison with the case of no purging and because at more than about 4 SCCM, the values of in the peaks of the hydrocarbon components are substantially constant. Under such a purging condition, it is possible for the suction pressure of the pump to be about 7.5 x 10⁻³ Torr to 2.5 x 10⁻² Torr.
- As Fig. 4 shows, when a small quantity of purge gas is supplied each peak value of component of the oil contained in the evacuated air is about one hundredth in comparison with the case of no purging, so that a clean vacuum state is provided. The quantity of purge gas according to the present invention is very small in comparison with the conventional purging method. For example, the quantity of purge gas according to the present invention will be compared with the quantity of purge gas according to the conventional purging method under the condition that the oil-sealed rotary vacuum pump evacuates by 240 ℓ/min.
- S is the pumping speed of the oil-sealed rotary vacuum pump, Q is the throughput of the vacuum pump, and P is the inlet pressure, a relation between these components is expressed by the following equation:
Q = SP (1)
When S is 240 ℓ/min and P is 0.1 Torr, the quantity of purge gas Q₁ supplied according to the conventional method is then expressed as follows.
Q₁ = 0.4 Torr ℓ/S ≒ 32 SCCM
As Fig. 4 shows, according to the present invention, an quantity of purge gas Q₂ enough for effective purging is 0.6 SCCM (when the ultimate pressure is at 7 x 10⁻³ Torr). Therefore, Q₂ (= 0.6 SCCM) is about one fifty-third in comparison with the conventional method. In consequence, the ultimate pressure of the vacuum pumping system according to the present invention can be lower than the pressure of 13 Pa (0.1 Torr) provided by the conventional purging method, and the vacuum state can be clean. How the interior of thespecimen chamber 3 can be made clean by the supply of a very small quantity of purge gas will be explained below. That is, according to the analysis: although the change in the pressure caused by the supply of a small quantity of purge gas is small, by the supply of the purge gas the Knudsen number increases, and the state of the evacuated flow changes from a molecular flow to an intermediate flow. As the result, the frequency in collision between the oil particles and the purge gas particles increases substantially, so that the backstreaming of the oil is impeded remarkably. Further, the supply of purging gas generates a flow toward the vacuum pump, and the oil particles are carried thereto. Thus, in the present embodiment, a vacuum state in which the oil contamination is decreased is provided by slight reconstructions of equipments used in the vacuum system. - Fig. 5 shows a second embodiment of the present invention in which the present invention is applied to a scanning electron microscope. Each of the parts shown in Fig. 5 and each of the parts shown in Fig. 1 which are identical with each other are denoted by the identical reference numeral. In this embodiment, the purge gas supply means 40 includes a
mass flow controller 44 for controlling a flow rate of purge gas, instead of theorifice 42 included in themeans 40 in the first embodiment. - In the present embodiment, since the flow rate of purge gas is always measured and controlled, the amount of purge gas does not change if the pressure at the inlet of the mass flow controller changes, so that the variation of pressure in vacuum system is very small.
- Fig. 6 shows a third embodiment of the present invention in which the present invention is applied to a scanning electron microscope. In this embodiment, the purge gas supply means 40 includes a
microflow supply valve 45, amicroflow meter 46, apurge gas source 47 and apurge gas pipe 41, and the purge gas is supplied not from the atmosphere but from thepurge gas source 47. In this embodiment, the main components of residual gas are supplied from thepurge gas source 47, so that the specimen can be surrounded by a desired gas as shown in Fig. 4. - Fig. 7 shows a fourth embodiment of the present invention in which the present invention is applied to a scanning electron microscope. In this embodiment, the purge gas supply means 40 includes a
microflow meter 46 which operates as a purging checker for checking whether or not a purge gas is flowing. Themicroflow meter 46 generates a signal for closing themanifold gate valve 22, thebypass valve 37 and thestop valve 33 when the quantity of purge gas is less than a predetermined level so that the oil contamination is prevented. The generated signal is transmitted through a valvecontrol signal line 48. This system improves the reliability of the system. - Fig. 8 shows a fifth embodiment of the present invention in which the present invention is applied to a scanning electron microscope. This embodiment employs a
Pirani gauge 34 as the purging checker. When the flow rate of purge gas reduces to a predetermined value or below, the ultimate pressure of the second oil-sealedrotary vacuum pump 30 lowers, and oil contamination increases. The vacuum pressure which is the predetermined value or below is detected by thePirani gauge 34 arranged in thesuction pipe 32 between the specimen exchange chamber and thesecond vacuum pump 30, and thePirani gauge 34 generates a signal to close themanifold gate valve 22, thebypass valve 37, and thestop valve 33. According to the present embodiment, the state in the inlet side of thesecond vacuum pump 30 is checked, so the reliability of the system is improved. - Fig. 9 shows a sixth embodiment of the present invention in which the present invention is applied to a scanning electron microscope. This embodiment includes, as a purging checker,
optical fiber cables 49 for detecting the clogging of themicroflow orifice 42, and adetector 50 for judging whether the orifice clogs up or not and for generating a signal to open or close the valves. Theoptical fibers 49 face each other at an end of themicroflow orifice 42. A ray of light inserted into an end of theoptical fiber 49 is detected by thedetector 50 when the purge gas flows through theorifice 42. However, if themicroflow orifice 42 is clogged by a foreign substance, the ray of light is interrupted, and no light is detected by thedetector 50. Since oil contamination increases when no purge gas is supplied, thedetector 50 judges whether the orifice clogs up or not and generates the signal for closing themanifold gate valve 22, thebypass valve 37 and thestop valve 33. In this embodiment, the clogging of themicroflow orifice 42 is always monitored, so that the reliability of the system is improved. - Fig. 10 shows a seventh embodiment of the present invention in which the present invention is applied to a scanning electron microscope. This embodiment includes a purge gas supply means 40 for supplying a controlled quantity of purge gas to the inlet side of the second oil-sealed
rotary vacuum pump 30 according to the pressure of the inlet side of the second oil-sealedrotary vacuum pump 30. The purge gas supply means 40 in this embodiment includes amicroflow supply valve 45, amicroflow meter 46, apurge gas source 47, apressure signal line 52, a microflow valvecontrol signal line 53 and amicroflow valve controller 51. In this embodiment, thePirani gauge 34 measures the pressure of the inlet side of the second oil-sealedrotary vacuum pump 30, generates a signal in accordance with the measured pressure and transmits the signal through thepressure signal line 52 to themicroflow valve controller 51. According to the transmitted signal, themicroflow valve controller 51 generates and transmits a signal for controlling the opening degree of themicroflow supply valve 45 through the microflow valvecontrol signal line 53 to themicroflow supply valve 45 so that the opening degree of themicroflow supply valve 45 increases or decreases in accordance with a difference between the measured pressure and the predetermined pressure. When the measured pressure is larger than the predetermined pressure, themicroflow valve controller 51 generates the signal for decreasing the opening degree of themicroflow supply valve 45. When the measured pressure is smaller than the predetermined pressure, themicroflow valve controller 51 generates the signal for increasing the opening degree of themicroflow supply valve 45. When the measured pressure is equal to the predetermined pressure, themicroflow valve controller 51 generates the signal for maintaining the opening degree of themicroflow supply valve 45 as it is. As described above, the pressure of the inlet side of the second oil-sealedrotary vacuum pump 30 is maintained within a suitable range. As in this embodiment the quantity of the supplied purge gas is automatically controlled, the reriability and economical efficiency of the system are improved. - In the above-described embodiments, the present invention is applied to a scanning electron microscope. However, the present invention can also be applied to a transmission type electron microscope, a mass spectrometer or an ion microanalyzer.
- As the above description shows, since the backstreaming of the oil used in the oil-sealed rotary vacuum pump toward the inlet side of the vacuum pump is suppressed when the air in the specimen exchange chamber is evacuated by the oil-sealed rotary vacuum pump to the ultimate pressure of the pump, a clean vacuum state is provided in the specimen exchange chamber, further the specimen chamber is not contaminated with the oil when a specimen is delivered into the specimen chamber, so that an analysis system employing electron in which oil contamination of the vacuum system is prevented can be provided.
Claims (11)
an electron generating source (2) for generating electron;
a specimen chamber (3) which is irradiated with the electron generated by said electron generating source (2);
a specimen exchange chamber (10) arranged on said specimen chamber (3) so that the specimen (9) is inserted into said specimen chamber (3) from said specimen exchange chamber (10);
a first oil-sealed rotary vacuum pump (26) for main pumping and roughing, said first oil-sealed rotary vacuum pump (26) is connected to said specimen chamber (3) to evacuate air in said specimen chamber (3);
a second oil-sealed rotary vacuum pump (30) connected through a suction pipe (32) to said specimen exchange chamber (10) to evacuate air in said specimen exchange chamber (10); and
a purge gas supply means (40) for supplying a small quantity of purge gas to said suction pipe (32) of said second oil-sealed rotary vacuum pump (30).
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62324009A JP2607572B2 (en) | 1987-12-23 | 1987-12-23 | Analysis device and method using charged particles |
JP324009/87 | 1987-12-23 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0321925A2 true EP0321925A2 (en) | 1989-06-28 |
EP0321925A3 EP0321925A3 (en) | 1990-04-11 |
EP0321925B1 EP0321925B1 (en) | 1997-03-26 |
Family
ID=18161110
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP88121303A Expired - Lifetime EP0321925B1 (en) | 1987-12-23 | 1988-12-20 | Apparatus for analysis employing electron |
Country Status (4)
Country | Link |
---|---|
US (1) | US4889995A (en) |
EP (1) | EP0321925B1 (en) |
JP (1) | JP2607572B2 (en) |
DE (1) | DE3855843T2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1515359A1 (en) * | 2003-09-12 | 2005-03-16 | ICT Integrated Circuit Testing Gesellschaft für Halbleiterprüftechnik mbH | Chamber with low electron stimulated desorption |
Families Citing this family (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0348759A (en) * | 1989-07-18 | 1991-03-01 | Nec Corp | Fluorescent x-ray analysis apparatus |
DE4136950A1 (en) * | 1991-11-11 | 1993-05-13 | Pfeiffer Vakuumtechnik | MULTI-STAGE VACUUM PUMP SYSTEM |
DE10032607B4 (en) * | 2000-07-07 | 2004-08-12 | Leo Elektronenmikroskopie Gmbh | Particle beam device with a particle source to be operated in ultra-high vacuum and a cascade-shaped pump arrangement for such a particle beam device |
GB0322889D0 (en) * | 2003-09-30 | 2003-10-29 | Boc Group Plc | Vacuum pump |
US7112803B2 (en) * | 2004-07-23 | 2006-09-26 | Applied Materials, Israel, Ltd. | Beam directing system and method for use in a charged particle beam column |
JP5016988B2 (en) * | 2007-06-19 | 2012-09-05 | 株式会社日立ハイテクノロジーズ | Charged particle beam apparatus and vacuum startup method thereof |
US8987664B2 (en) * | 2013-02-07 | 2015-03-24 | Shimadzu Corporation | Mass spectrometry device |
JP6207344B2 (en) * | 2013-10-30 | 2017-10-04 | 日本電子株式会社 | Charged particle beam equipment |
DE112014006916B4 (en) * | 2014-10-09 | 2021-01-28 | Hitachi High-Tech Corporation | Device operating with a charged particle beam and electron microscope |
JP6407411B2 (en) * | 2015-04-15 | 2018-10-17 | 株式会社日立ハイテクノロジーズ | Charged particle beam device and vacuum exhaust method thereof |
DE102016114983A1 (en) * | 2016-08-12 | 2018-02-15 | Pfeiffer Vacuum Gmbh | vacuum system |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS63285924A (en) * | 1987-05-19 | 1988-11-22 | Hitachi Ltd | Device for manufacturing semiconductor |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3385102A (en) * | 1966-04-21 | 1968-05-28 | Nat Res Corp | Rapid cycle leak detection of plural test pieces |
NL7010108A (en) * | 1969-09-30 | 1971-04-01 |
-
1987
- 1987-12-23 JP JP62324009A patent/JP2607572B2/en not_active Expired - Fee Related
-
1988
- 1988-12-20 US US07/286,848 patent/US4889995A/en not_active Expired - Lifetime
- 1988-12-20 DE DE3855843T patent/DE3855843T2/en not_active Expired - Fee Related
- 1988-12-20 EP EP88121303A patent/EP0321925B1/en not_active Expired - Lifetime
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS63285924A (en) * | 1987-05-19 | 1988-11-22 | Hitachi Ltd | Device for manufacturing semiconductor |
Non-Patent Citations (2)
Title |
---|
JAPANESE JOURNAL OF APPLIED PHYSICS, Suppl. 2, pt. 1, 1974, pages 249-252, Tokyo, JP; N. YOSHIMURA et al.: "A new vacuum system for an electron microscope" * |
THE JOURNAL OF VACUUM SCIENCE AND TECHNOLOGY, vol. 8, no. 1, 1971, pages 299-307, American Institute of Physics, New York, US; D.J. SANTELER: "The use of diffusion pumps for obtaining ultraclean vacuum environments" * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1515359A1 (en) * | 2003-09-12 | 2005-03-16 | ICT Integrated Circuit Testing Gesellschaft für Halbleiterprüftechnik mbH | Chamber with low electron stimulated desorption |
WO2005027175A1 (en) * | 2003-09-12 | 2005-03-24 | Ict Integrated Circuit Testing Gesellschaft Fur Halbleiterpruftechnik Mbh | Chamber with low electron stimulated desorption |
Also Published As
Publication number | Publication date |
---|---|
DE3855843D1 (en) | 1997-04-30 |
JPH01166457A (en) | 1989-06-30 |
EP0321925B1 (en) | 1997-03-26 |
US4889995A (en) | 1989-12-26 |
EP0321925A3 (en) | 1990-04-11 |
DE3855843T2 (en) | 1997-11-06 |
JP2607572B2 (en) | 1997-05-07 |
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